CN102992611A - Method for manufacturing glass base material - Google Patents

Method for manufacturing glass base material Download PDF

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Publication number
CN102992611A
CN102992611A CN2012103327961A CN201210332796A CN102992611A CN 102992611 A CN102992611 A CN 102992611A CN 2012103327961 A CN2012103327961 A CN 2012103327961A CN 201210332796 A CN201210332796 A CN 201210332796A CN 102992611 A CN102992611 A CN 102992611A
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core tube
furnace core
stacked body
sintering
glass granules
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CN102992611B (en
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幅崎利已
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/014Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01446Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Thermal Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

The invention provides a method for manufacturing a glass base material, where the interior of a furnace core tube is reliably prevented from being polluted by avoiding invasion of foreign matters from the outside during non-working time. In the method for manufacturing a glass base material, a glass particle stack body (13) formed by stacked glass particles is hung in the furnace core tube (11) and is heated from the exterior of the furnace core tube (11) so as to be dehydrated and sintered. During the non-working time except the dehydrating and sintering time, the standby temperature in the furnace core tube (11) is kept to be higher than or equal to 700 DEG C, so as to prevent invasion of foreign matters.

Description

The manufacture method of base glass material
Technical field
The present invention relates to a kind of manufacture method of base glass material, it makes glass granules stacked body dehydration sintering by the glass granules stacked body heating that stacking glass granules is formed.
Background technology
In the manufacture method of common base glass material, by gas phase synthesis methods such as VAD method or OVD methods, make for example silicon chlorides (SiCl of unstripped gas 4) etc. in oxyhydrogen flame, carry out the flame decomposition reaction, be silicon-dioxide (SiO thereby generate glass granules 2), by being stacked on, this glass granules makes glass granules stacked body (stacking operation) on the initial glass rod in the Reaktionsofen.
For above-mentioned glass granules stacked body, with chlorine (Cl 2) and the mixed gas of helium (He) import in the dehydration-sintering furnace, be heated to about 1300 ℃ of degree and make glass granules stacked body dehydration (dehydration procedure), afterwards, carry out sintering by the glass granules stacked body is heated to about 1550 ℃ of degree in helium, thereby carry out transparent glass (sintering circuit).
Usually, as the material of the furnace core tube of the dehydration-sintering furnace that uses in above-mentioned dehydration, the sintering circuit, mainly use quartzy (quartzy furnace core tube) and carbon (carbon furnace core tube) (for example, with reference to patent documentation 1).
Patent documentation 1: TOHKEMY 2005-187303 communique
Summary of the invention
But if known above-mentioned quartzy furnace core tube and the carbon furnace core tube of using under the same conditions made base glass material, the quality of each base glass material that then produces is different.Namely, if come drawing optical fiber and the two compared based on each base glass material that produces, then can confirm following situation, namely, compare with the optical fiber that obtains based on the base glass material that is produced by quartzy furnace core tube, the generation frequency of the abnormity point such as the optical fiber broken string that obtains based on the base glass material that is produced by the carbon furnace core tube or wire diameter fluctuation is higher.
Therefore, the contriver thinks that this is owing to compare with the base glass material that is produced by quartzy furnace core tube, more the causing of amount of the impurity of the mother metal surface adhesion of the base glass material that is produced by the carbon furnace core tube, the difference of creating conditions during to quartzy furnace core tube and carbon furnace core tube has been carried out probe, standby temperature when finding inoperative particularly exerts an influence to the abnormity point occurrence frequency, thereby has proposed the present invention.
The object of the present invention is to provide a kind of manufacture method of base glass material, it prevents when inoperative especially from intrusions such as the impurity of outside and can prevent reliably that furnace core tube inside is contaminated.
The manufacture method that can solve the base glass material involved in the present invention of above-mentioned problem is, the glass granules stacked body that stacking glass granules is formed is hung in furnace core tube, heat and the sintering that dewaters from this furnace core tube outside to above-mentioned glass granules stacked body, the manufacture method of this base glass material is characterised in that, during inoperative except above-mentioned dehydration sintering the time, the standby temperature of above-mentioned furnace core tube inside is remained more than or equal to 700 ℃, invade to prevent impurity.
In addition, the preferred above-mentioned furnace core tube of the manufacture method of base glass material involved in the present invention is the carbon goods.
The effect of invention
Manufacture method according to base glass material involved in the present invention, by when the inoperative except dehydration is during sintering, the standby temperature of furnace core tube inside is remained more than or equal to 700 ℃, thereby in furnace core tube, produce all the time upstream, prevent the intrusion from the impurity of outside, can prevent reliably that furnace core tube inside is by contaminating impurity.The abnormity point such as the broken string that produces in the optical fiber in the time of therefore, can be with wire drawing or wire diameter fluctuation suppress to be bottom line.
Description of drawings
Fig. 1 is the synoptic diagram of an example of expression dehydration agglomerating plant, and this dehydration agglomerating plant is used for implementing the manufacture method of base glass material involved in the present invention.
Embodiment
Below, a preferred implementation of the manufacture method of base glass material involved in the present invention is described.
As shown in Figure 1, the dehydration agglomerating plant 10 of the manufacture method of the base glass material of enforcement present embodiment, outer circumferential side has well heater 12 at the middle part of furnace core tube 11.The heat that time per unit applies to glass granules stacked body 13 can be easily controlled in this dehydration agglomerating plant 10 use in the dehydration procedure of glass granules stacked body 13, sintering circuit etc.
The furnace core tube 11 of dehydration agglomerating plant 10 is carbon goods.Be hung with glass granules stacked body 13 in furnace core tube 11, this glass granules stacked body is to utilize flame hydrolysis to make glass granules be stacked on porous plastid on the initial glass rod 14.The upper end of glass granules stacked body 13 is fixed on the grip part 15.
Grip part 15 is via support stick 16 and hoisting appliance 17 combinations.Support stick 16 can be by mobile along the vertical direction by the hoisting appliance 17 of control device 18 controls.Hoisting appliance 17 as required, makes glass granules stacked body 13 be moved upward from the below with respect to the heating region of well heater 12 with the lift velocity that sets when dehydration or sintering.
The upper end of furnace core tube 11 is provided with loam cake 19.But be inserted with support stick 16 on this loam cake 19, this support stick is support glass particulate stacked body 13 rotatably free lifting.In addition, when changing glass granules stacked body 13, loam cake 19 can be unloaded from furnace core tube 11.
The bottom of furnace core tube 11 is provided with processes gas supply pipe 20.Process gas supply pipe 20 in furnace core tube 11 from this, by not shown gas apparatus for controlling of supply, when dehydration, supply with the mixed gas of chlorine and helium and process gas, when sintering, supply with helium.
The top of furnace core tube 11 is provided with the processing gas exhaust pipe 21 that is connected on the not shown exhaust gas treatment device.By above-mentioned exhaust gas treatment device, 11 outer discharge chlorine, helium and dehydration from this processing gas exhaust pipe 21 to furnace core tube and moisture of producing etc.
In the manufacture method of the base glass material of present embodiment, when dehydration or sintering, in dehydration agglomerating plant 10, the outside from the furnace core tube 11 of carbon system is heated to glass granules stacked body 13 respectively about 1300 ℃, 1600 ℃ by well heater 12.
And, during inoperative except above-mentioned dehydration or sintering the time, by carrying out temperature treatment by control device 18 control heaters 12, make the standby temperature of furnace core tube 11 inside more than or equal to 700 ℃.At this moment, in furnace core tube 11, supply with the nitrogen (N of specified amount from processing gas supply pipe 20 by the gas apparatus for controlling of supply 2).In addition, refer to during inoperative described here, when the replacing operation of glass granules stacked body 13, wait for put into next glass granules stacked body during etc., when not comprising the safeguarding of furnace core tube 11 etc.
Remain more than or equal to 700 ℃ by the standby temperature with furnace core tube 11 inside, can make the upstream 22 of furnace core tube 11 interior generation nitrogen.Utilize this upstream 22, can prevent from invading from the impurity on furnace core tube 11 tops.In addition, can think to produce the upstream 22 with abundant flow velocity under less than 700 ℃ standby temperature, can't stop fully from the impurity of outside and invade.In addition, also can be with the standby temperature increase to dehydration or the Heating temperature during sintering, but Heating temperature is higher, and electric power consumption is just larger, cost of idleness.
Below, dehydration, the sintering method of glass granules stacked body described.
(mother metal 1 is installed)
Under the temperature with furnace core tube 11 inside remains more than or equal to 700 ℃ state, as shown in Figure 1, glass granules stacked body 13 is inserted in the furnace core tube 11, hang in the mode that glass granules stacked body 13 is arranged on the appropriate position in the furnace core tube 11.
(dehydration/sintering 1)
Then, glass granules stacked body 13 is heated to about 1300 ℃ and dewater in the mixed gas of chlorine and helium.Then, for glass granules stacked body 13, in helium, utilize well heater 12 that furnace core tube 11 is heated to about 1600 ℃, and carry out aligned in position so that the upper end of glass granules stacked body 13 becomes near the mode of the height in the lower end of well heater 12, by hoisting appliance 17 glass granules stacked body 13 is risen with the setting speed of regulation.
Glass granules stacked body 13 carries out sintering from top to the bottom order through the heating region of well heater 12 formation, behind the topmost (end position) in the arrival furnace core tube 11, finishes sintering circuit.Thus, glass granules stacked body 13 along its length direction from top to the bottom by heated in sequence, thereby transparence.
(mother metal is installed 2/ standby 1)
Then, with the base glass material after the transparence after furnace core tube 11 interior taking-ups, next glass granules stacked body 13 is inserted in the furnace core tubes 11, and is installed in the furnace core tube 11.
In this mother metal installation exercise, when being inoperative, carry out temperature treatment by control device 18, so that the standby temperature of furnace core tube 11 inside remains more than or equal to 700 ℃.At this moment, at the replacing position of loam cake 19, the upper end opening of furnace core tube 11, but since the standby temperature more than or equal to 700 ℃, so furnace core tube 11 interior generation upstreams 22.Utilize this upstream 22 and stop from the impurity of the upper end open of furnace core tube 11 and invade.In addition, until during putting into the standby of next mother metal, also since the standby temperature more than or equal to 700 ℃, thereby at furnace core tube 11 interior generation upstreams 22, can stop intrusion impurity from the gap of upper end etc.
(dehydration/sintering 2)
The 2nd glass granules stacked body 13 and above-mentioned (dehydration/sintering 1) are dewatered and sintering in the same manner.
(mother metal is installed 3/ standby 2)
When the base glass material after the 2nd transparence being taken out to the inoperative that 13 of the 3rd glass granules stacked bodies are installed, with above-mentioned (mother metal is installed 2/ standby 1) in the same manner, carry out temperature treatment so that the standby temperature of furnace core tube 11 inside remains more than or equal to 700 ℃.And, repeat to dewater, sintering, mother metal are installed, each operation of standby, until dehydration and the sintering of last glass granules stacked body 13 are finished.
As mentioned above, according to the manufacture method of the base glass material of present embodiment, during inoperative except the dehydration sintering time, the standby temperature that makes furnace core tube 11 inside is more than or equal to 700 ℃ temperature treatment.Thus, at furnace core tube 11 interior generation upstreams 22, can utilize this upstream 22 to prevent that impurity is to furnace core tube 11 interior intrusions.
In addition, the manufacture method of base glass material of the present invention is not limited to above-mentioned embodiment, can freely suitably be out of shape, improvement etc.For example, in the present embodiment, be illustrated as an example of the carbon furnace core tube example, but also can be applied to quartzy furnace core tube.In addition, quartzy furnace core tube is being heated in the situation of high temperature (more than or equal to 1000 ℃), quartzy furnace core tube cristobalite (devitrification phenomenon) occurs and changes, be less than or equal to original lesser temps (300 ℃) if under this state, return to, then break, therefore, for the situation of quartzy furnace core tube, usually when inoperative, also to keep higher standby temperature.But this is in order to prevent that as mentioned above furnace core tube from breaking, and is not to prevent that impurity from invading in the furnace core tube is that purpose is implemented.
In addition, in the present embodiment, take with the local heating of furnace core tube and the mobile along the vertical direction zone melting stove of glass granules stacked body is illustrated as example, but also can be applicable to the soaking pit with the whole heating of furnace core tube.In addition, utilizing that other stove and accessorys dewater, in the situation of sintering, also can be applicable to each stove and accessory.
(embodiment)
Below, an embodiment of the manufacture method of base glass material of the present invention is described.
As described in Table 1, for embodiment and Comparative Examples, all the standby temperature in the carbon furnace core tube is changed, under each standby temperature, carry out the installation exercise of glass granules stacked body, 1~several these glass granules stacked bodies are dewatered and sintering.And, each base glass material of making is carried out wire drawing and be wound on the bobbin, each bobbin is measured transmission loss, determine size and the fluctuation of loss.
Particularly, remain more than or equal to 700 ℃ mode with the standby temperature in an embodiment and carry out temperature treatment, in Comparative Examples, remain less than 700 ℃ mode with the standby temperature and carry out temperature treatment, and dewater as mentioned above and sintering, thereby make base glass material.Then, for the bobbin behind drawing optical fiber from each base glass material and the coiling, measure transmission loss to measure wavelength 1550nm, and add up the measurement result of the transmission loss under each standby temperature condition.Finally, obtained the result shown in the table 1.
Table 1
Figure BDA00002118035500061
According to table 1 as can be known, in remaining the standby temperature in the furnace core tube more than or equal to 700 ℃ embodiment 1~4, the value of transmission loss is less by 0.18~0.22(dB/km), and the fluctuation of transmission loss is also less.Infer that this is owing to produce upstream in furnace core tube, utilize this upstream to prevent that impurity from invading in furnace core tube, produce the less base glass material of frequency and cause thereby made abnormity point.
Relative therewith, the standby temperature in making furnace core tube is less than in 700 ℃ the Comparative Examples 1,2, and it is large that the value of transmission loss becomes, and is 0.21~0.30(dB/km), and it is large that the fluctuation of transmission loss also becomes.Think that its reason is, because the standby temperature in the furnace core tube is less than 700 ℃, so do not produce sufficient upstream, impurity is invaded in the furnace core tube and is sticked on the base glass material.

Claims (2)

1. the manufacture method of a base glass material, in the method, the glass granules stacked body that stacking glass granules is formed is hung in furnace core tube, from this furnace core tube outside to described glass granules stacked body heating and the sintering that dewaters,
It is characterized in that,
During inoperative except described dehydration sintering the time, the standby temperature of described furnace core tube inside is remained more than or equal to 700 ℃, invade to prevent impurity.
2. the manufacture method of base glass material according to claim 1 is characterized in that,
Described furnace core tube is the carbon goods.
CN201210332796.1A 2011-09-09 2012-09-10 The manufacture method of base glass material Active CN102992611B (en)

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JP2011196814A JP2013056808A (en) 2011-09-09 2011-09-09 Method for producing glass preform

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112225448A (en) * 2020-10-22 2021-01-15 江苏亨通光导新材料有限公司 Helium-chlorine mixed gas circulation system for sintering optical fiber perform
CN112694248A (en) * 2015-09-30 2021-04-23 住友电气工业株式会社 Lifting device for glass base material

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111960658B (en) * 2020-09-20 2023-08-22 连云港三明石英制品有限公司 Special OVD sintering quartz furnace with core tube positioning clamp
CN113651526B (en) * 2021-08-02 2023-02-10 富通集团(嘉善)通信技术有限公司 Machining process of core rod

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1040355A (en) * 1988-08-16 1990-03-14 住友电气工业株式会社 The process furnace of the first base of optical fiber glass and manufacturing glass is the method for base just
CN1076430A (en) * 1991-12-16 1993-09-22 住友电气工业株式会社 The process for heating vitrification of porous preform for optical fiber
US5259856A (en) * 1989-09-06 1993-11-09 Sumitomo Electric Industrial, Ltd. Method of producing glass preform in furnace for heating glass
JPH06112145A (en) * 1992-09-28 1994-04-22 Matsushita Electron Corp Trichloroethane cleaning method for furnace tube of heat treating furnace

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1040355A (en) * 1988-08-16 1990-03-14 住友电气工业株式会社 The process furnace of the first base of optical fiber glass and manufacturing glass is the method for base just
US5259856A (en) * 1989-09-06 1993-11-09 Sumitomo Electric Industrial, Ltd. Method of producing glass preform in furnace for heating glass
CN1076430A (en) * 1991-12-16 1993-09-22 住友电气工业株式会社 The process for heating vitrification of porous preform for optical fiber
JPH06112145A (en) * 1992-09-28 1994-04-22 Matsushita Electron Corp Trichloroethane cleaning method for furnace tube of heat treating furnace

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112694248A (en) * 2015-09-30 2021-04-23 住友电气工业株式会社 Lifting device for glass base material
CN112694248B (en) * 2015-09-30 2023-02-03 住友电气工业株式会社 Lifting device for glass base material
CN112225448A (en) * 2020-10-22 2021-01-15 江苏亨通光导新材料有限公司 Helium-chlorine mixed gas circulation system for sintering optical fiber perform

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